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US9464009B2 - Removal of urea and ammonia from exhaust gases - Google Patents
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US9464009B2 - Removal of urea and ammonia from exhaust gases - Google Patents

Removal of urea and ammonia from exhaust gases Download PDF

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Publication number
US9464009B2
US9464009B2 US13/496,192 US201013496192A US9464009B2 US 9464009 B2 US9464009 B2 US 9464009B2 US 201013496192 A US201013496192 A US 201013496192A US 9464009 B2 US9464009 B2 US 9464009B2
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urea
uas
melt
ammonium sulphate
water
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US20120240649A1 (en
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Jozef Hubert Meessen
Pantelis Orfanidis
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Stamicarbon BV
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Stamicarbon BV
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Assigned to STAMICARBON B.V. reassignment STAMICARBON B.V. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MEESSEN, JOZEF HUBERT, ORFANIDIS, PANTELIS
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    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/54—Nitrogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/54—Nitrogen compounds
    • B01D53/58—Ammonia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/80—Semi-solid phase processes, i.e. by using slurries
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/12—Separation of ammonia from gases and vapours
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/22—Sulfites of ammonium
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
    • C05C3/005—Post-treatment
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C9/00—Fertilisers containing urea or urea compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
    • C07C273/14—Separation; Purification; Stabilisation; Use of additives
    • C07C273/16—Separation; Purification
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/50—Inorganic acids
    • B01D2251/506—Sulfuric acid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/40—Nitrogen compounds
    • B01D2257/406—Ammonia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602

Definitions

  • Urea dust and ammonia are known to be present in exhaust gases from urea plants, urea granulation towers, urea prilling towers and chemical fertilizer plants. Such plants in particular release waste air streams that contain dust and ammonia resulting from various process steps. This air stream must be purified before being passed into the environment or recycled back into the process. Such waste air stream result in particular from granulation, prilling and product cooling process steps.
  • JP9227493 describes a method for recovery of urea dust and ammonia from such a gas stream by contacting said gas stream with an aqueous sulphuric acid solution, thus forming an acid solution of ammonium sulphate and urea.
  • a disadvantage of the known process is, that the resulting product is a solution, which can hardly be used as a fertilizer due to its high transport costs.
  • JP9227493 Another problem of the method described in JP9227493 is that the resulting solution is an acidic solution, which is not only a disadvantage for the soil wherein it is used as a fertilizer, but it results in corrosion in metal equipment used to concentrate, handle and transport the acidic solution, unless special, high cost, materials of construction are used for such metal equipment.
  • This problem can be solved, by adding ammonia to the acidic solution before the acidic solution is concentrated, thus forming a neutralized solution of ammonium sulphate and urea in water.
  • the neutralized solution is concentrated by vaporization of at least part of the water phase, thus forming water vapor and a melt comprising less than 5 wt % of water.
  • the vaporization is carried out in more than one step until the amount of water is less than 5 wt %. This allows reducing the amount of water in the melt to less than 1 wt %, and even to less than 0.3 wt %.
  • the melt is transferred into urea and ammonium sulphate comprising solid particles.
  • This process can be carried out in a granulator, or prilling tower. However this would reintroduce (on a smaller scale) the problem of ammonia and dust loaded air. Therefore this process is preferably carried out in a pelletizer, comprising a feeding device, a solidification/cooling belt and a device to remove the formed pellets from the belt, by feeding a urea-comprising liquid to the feeding device from which droplets of the urea-comprising liquid are dosed to the belt, whereon the urea-comprising droplets solidify, where after the formed urea-comprising particles are removed from the belt.
  • the belt is cooled from the other side, preferably by means of cooling water.
  • FIG. 1 is a schematic system for implementing an embodiment of the present invention.
  • FIG. 2 is schematic system for implementing of another embodiment of the present invention.
  • FIG. 3 is a schematic system for implementing of a further embodiment of the present invention.
  • FIG. 1 A system for implementing the method of the invention is shown in FIG. 1 .
  • a gas stream comprising air, urea and ammonia ( 11 ) is contacted in a scrubber ( 1 ) with an aqueous sulphuric acid solution ( 12 ), thus forming an acidic solution of urea and ammonium sulphate.
  • Scrubber ( 1 ) can be selected from any of the wet-type scrubbers well known in the industry. It may, for instance, be selected from the type of scrubbers as summarized in Chemical Engineers Handbook (Perry and Chilton), fifth edition, page 20-94 to 20-103. Stream 11 usually has a relative high temperature (70-110° C.), and may be rather dry. As a result of this, quite some water may evaporate in the scrubber. In many cases it therefore will be required to add make-up water ( 15 ) to the scrubber in order to assure that the concentration of urea and ammonium sulphate in the liquid phase in the scrubber remains below the solubility limits. Depending on the type of scrubber selected, circulation of acidic urea/ammonium sulphate (UAS) solution over the scrubber (not shown in the figure) may be required for proper removal of ammonia and dust from the air stream.
  • UAS acidic urea/ammonium sulphate
  • the cleaned air leaves the scrubber via line 18 .
  • the acidic solution of urea and ammonium sulphate is passed through line ( 21 ) to concentration unit ( 2 ), which may comprise at least one concentrator Water vapor leaves the concentration unit ( 2 ) via line ( 16 ).
  • concentration unit ( 2 ) the acidic solution of urea and ammonia is concentrated to a melt, comprising less than 5 wt % of water.
  • the concentration unit ( 2 ) may consist of one or more evaporators in parallel or in series. These evaporators may be selected from evaporators, as they are well known in the process industry. They may, for instance, be selected from the evaporators as summarized in Chemical Engineers Handbook (Perry and Chilton), fifth edition, pages 11-27 to 11-38.
  • Urea is vulnerable for decomposition (e.g. hydrolyses and biuret formation) at high temperatures and at long residence time.
  • the evaporators are usually selected from the types ‘falling film’ or ‘Long tube vertical’ (refer to FIG. 11-16 in Chemical Engineers Handbook (Perry and Chilton), fifth edition) since they offer low residence time.
  • the evaporators preferably are operated under vacuum, in order to minimize the required temperature.
  • the vacuum in the evaporators can be maintained using a system of vacuum condensers and steam-jet ejectors (not shown in the figure), or other systems, that are well known in the industry.
  • the concentrated UAS melt leaves the concentration unit via line ( 22 ) to mixer ( 3 ).
  • Solid ammonium sulphate is also introduced into the mixer ( 3 ), in order to increase the ammonium sulphate to urea ratio to the desired value.
  • the dosing of ammonium sulphate to mixer ( 3 ) is controlled in such a way that a stable ammonium sulphate to urea ratio is obtained in the final product ( 17 ).
  • Mixer ( 3 ) may be selected from any of the solid/liquid mixers well known in the industry. It may e.g. be selected from the mixers as summarized in Chemical Engineers Handbook (Perry and Chilton), fifth edition, pages 19-3 to 19-25.
  • Selection of the mixer mainly is depending on the required ammonium sulphate to urea ratio. In case low concentrations of ammonium sulphate are required, then the solid concentration in slurry ( 23 ) will be low. In that case it will be sufficient to select the mixer from the class of ‘agitating mixers’. In case higher concentrations of ammonium sulphate are required, then the mixer more effectively can be selected of the class of ‘paste and viscous material mixing’ equipment. From the mixer slurry of solid ammonium sulphate in a urea/ammonium sulphate (UAS) + melt is transported via line ( 23 ) to the solid shaping step ( 4 ).
  • UAS urea/ammonium sulphate
  • the solid shaping step ( 4 ) may consist of granulation, prilling or pelletizing. It is of special advantage to select pelletizing as solid shaping process, since such a pelletizing process does not result in dust and ammonia loaden off-gas as is the case with prilling and granulation processes. An example of such a pelletizing process is described in WO 2006/111331 A1.
  • FIG. 2 shows a system for implementing the method of the invention, wherein ammonia or ammonia water ( 14 ) is added to the acid solution in a neutralizer ( 5 ) before the acidic solution ( 21 ) is concentrated, thus forming a neutralized solution of urea and ammonium sulphate in water that is passed through line ( 24 ) to the concentration unit ( 2 ).
  • the neutralizing process ( 5 ) may be accommodated in a mixing vessel with agitator, as well known in the industry. Taking into account the strong chemical affinity between sulphuric acid and ammonia, the neutralizing process may even be accommodated in a much simpler way, e.g. by supplying turbulent flow and sufficient residence time in the process line that transports UAS solution 24 to the concentration unit ( 2 ).
  • FIG. 3 shows a further embodiment of the invention.
  • the embodiment as shown in FIG. 3 offers special advantages over those as shown in FIGS. 1 and 2 , in case the required ammonium sulphate to urea ratio in the final UAS product is limited.
  • a gas stream comprising air, urea and ammonia ( 11 ) is contacted in a scrubber ( 1 ) with an aqueous sulphuric acid solution ( 12 ), thus forming an acidic solution of urea and ammonium sulphate.
  • the cleaned air leaves the scrubber via ( 18 ).
  • Make-up water is introduced into the scrubber via ( 15 ), in such an amount that no solids are formed in the streams ( 21 ) and ( 24 )
  • the formed acidic solution of urea and ammonium sulphate leaves the scrubber via ( 21 ), to be introduced in mixer ( 3 ).
  • NH 3 (or ammonia water) is introduced into mixer ( 3 ) via line ( 14 ) in such an amount that the excess sulphuric acid present in ( 21 ) is neutralized.
  • Additional solid ammonium sulphate is added to mixer ( 3 ) via line ( 13 ).
  • Mixer ( 3 ) is an agitated vessel, where proper agitation ensures that all of the solid ammonium sulphate that is added to the mixer is dissolved before the enriched UAS solution leaves the mixer via ( 24 ) to concentration unit ( 2 ).
  • the UAS solution is concentrated to such an extend that the UAS melt leaving the concentration unit via ( 23 ) has a water content of less the 5% by weight.
  • This concentrated melt is transformed into a solid UAS product in solid shaping unit ( 4 ) in the same way as described for FIG. 1 .
  • FIG. 3 offers the advantage that the process steps (5, neutralizer) and ( 3 , mixer) now are combined in one step ( 3 , mixer). This offers the advantage of lower capital investment for the process as described under FIG. 3 .
  • An advantage of the process as described under FIG. 2 as compared to the process as described under FIG. 3 is that the ammonium sulphate concentration in concentration step ( 2 ) can be higher without risking line blockage. Therefore the application of the process as described under FIG.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biomedical Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Fertilizers (AREA)
  • Treating Waste Gases (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US13/496,192 2009-09-16 2010-08-10 Removal of urea and ammonia from exhaust gases Active US9464009B2 (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
EP09170447.8 2009-09-16
EP09170447A EP2301917A1 (fr) 2009-09-16 2009-09-16 Élimination de l'urée et de l'ammoniac de gaz d'échappement
EP09170447 2009-09-16
PCT/EP2010/061588 WO2011032786A1 (fr) 2009-09-16 2010-08-10 Élimination d'urée et d'ammoniac de gaz d'échappement

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2010/061588 A-371-Of-International WO2011032786A1 (fr) 2009-09-16 2010-08-10 Élimination d'urée et d'ammoniac de gaz d'échappement

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US14/098,496 Continuation US9556077B2 (en) 2009-09-16 2013-12-05 Removal of urea and ammonia from exhaust gases

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US20120240649A1 US20120240649A1 (en) 2012-09-27
US9464009B2 true US9464009B2 (en) 2016-10-11

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US13/496,192 Active US9464009B2 (en) 2009-09-16 2010-08-10 Removal of urea and ammonia from exhaust gases
US14/098,496 Active US9556077B2 (en) 2009-09-16 2013-12-05 Removal of urea and ammonia from exhaust gases
US15/421,265 Active US10640428B2 (en) 2009-09-16 2017-01-31 Removal of urea and ammonia from exhaust gases

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US15/421,265 Active US10640428B2 (en) 2009-09-16 2017-01-31 Removal of urea and ammonia from exhaust gases

Country Status (10)

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US (3) US9464009B2 (fr)
EP (2) EP2301917A1 (fr)
CN (1) CN102596901A (fr)
AR (1) AR079185A1 (fr)
BR (1) BR112012006029B1 (fr)
CA (1) CA2774246C (fr)
EA (1) EA021089B1 (fr)
MY (1) MY160240A (fr)
PL (1) PL2477961T5 (fr)
WO (1) WO2011032786A1 (fr)

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JP6306571B2 (ja) * 2012-05-03 2018-04-04 スタミカーボン・ベー・フェー 尿素製造プラント
EP2746244A1 (fr) * 2012-12-21 2014-06-25 Uhde Fertilizer Technology B.V. Procédé pour réduire l'opacité du panache détaché auto-orientable visible
ITMI20130847A1 (it) * 2013-05-24 2014-11-25 Saipem Spa Metodo e sistema per il recupero di solfato di ammonio da un flusso gassoso di un impianto urea
EP3020702A1 (fr) * 2014-11-12 2016-05-18 Casale SA Procédé de finition d'urée avec lavage à l'acide
CN107848903B (zh) 2015-07-06 2021-09-21 斯塔米卡邦有限公司 尿素产品的制粒
BR112019007135A2 (pt) * 2016-10-13 2019-07-02 Koch Agronomic Services Llc recuperação e reutilização de componentes dos fluxos de resíduos de acabamento de ureia
WO2018122377A1 (fr) 2016-12-30 2018-07-05 Yara International Asa Traitement des gaz d'échappement d'une installation d'urée
EP3562784B8 (fr) 2016-12-30 2022-12-07 Yara International ASA Procédé de traitement d'un flux de gaz contenant de la poussière d'urée et de l'ammoniac
EP3366670A1 (fr) * 2017-02-27 2018-08-29 Casale Sa Procédé et système de capture d'ammoniac à partir d'un gaz de purge d'une usine d'urea
DE102017203251A1 (de) * 2017-02-28 2018-08-30 Thyssenkrupp Ag Verfahren zur Reinigung der Abluft einer Granulierungsanlage zur Herstellung eines harnstoffhaltigen Granulats
CN107349872A (zh) * 2017-03-16 2017-11-17 重庆宝禾复合肥有限公司 一种用于化肥生产的高效造粒设备
JP6851869B2 (ja) * 2017-03-17 2021-03-31 東洋エンジニアリング株式会社 尿素の造粒方法
MY194352A (en) * 2018-06-05 2022-11-29 Mitsubishi Heavy Ind Eng Ltd Fertilizer production plant and fertilizer production method
EP3639916A1 (fr) 2018-10-18 2020-04-22 Yara International ASA Procédé et granulateur à lit fluidisé pour la production de granulés à partir d'une boue
WO2020235999A1 (fr) 2019-05-22 2020-11-26 Stamicarbon B.V. Traitement de gaz d'échappement provenant d'une finition d'urée
DE102019216931A1 (de) * 2019-11-04 2021-05-06 Thyssenkrupp Ag Verfahren und Anlage zur Herstellung von Harnstoffgranulat

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Publication number Priority date Publication date Assignee Title
US2902342A (en) * 1955-01-27 1959-09-01 Jr Bernard J Kerley Method and apparatus for producing ammonium salts
US3928015A (en) 1974-10-29 1975-12-23 Tennessee Valley Authority Manufacture of urea-ammonium sulate from sulfuric acid, ammonia, and urea
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AR079185A1 (es) 2012-01-04
US20140090433A1 (en) 2014-04-03
US10640428B2 (en) 2020-05-05
BR112012006029B1 (pt) 2022-03-22
US20170137330A1 (en) 2017-05-18
EP2477961A1 (fr) 2012-07-25
US20120240649A1 (en) 2012-09-27
EA201270417A1 (ru) 2012-08-30
PL2477961T3 (pl) 2016-10-31
EP2477961B1 (fr) 2016-04-20
CA2774246A1 (fr) 2011-03-24
EA021089B1 (ru) 2015-04-30
BR112012006029A2 (pt) 2021-08-17
US9556077B2 (en) 2017-01-31
EP2477961B2 (fr) 2023-12-06
EP2301917A1 (fr) 2011-03-30
CA2774246C (fr) 2016-06-28
CN102596901A (zh) 2012-07-18
MY160240A (en) 2017-02-28

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